Ammonia → Ethyl 3-amino-2-(4-methylphenyl)propyl(diethoxymethyl)phosphinate

HRID 542323노트

반응식

HRID 542323 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([CH2:22][N+:23]([O-])=O)[CH2:9][P:10]([CH:15]([O:19][CH2:20][CH3:21])[O:16][CH2:17][CH3:18])(=[O:14])[O:11][CH2:12][CH3:13])=[CH:4][CH:3]=1.N.[H][H]>C(O)C.[Ni]>[NH2:23][CH2:22][CH:8]([C:5]1[CH:4]=[CH:3][C:2]([CH3:1])=[CH:7][CH:6]=1)[CH2:9][P:10]([CH:15]([O:19][CH2:20][CH3:21])[O:16][CH2:17][CH3:18])(=[O:14])[O:11][CH2:12][CH3:13]

참가 물질

6

반응물 3

HCID 222AmmoniaHCID 14362829Ethyl 2-(4-methylphenyl)-3-nitropropyl(diethoxymethyl)phosphinateHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 14362835Ethyl 3-amino-2-(4-methylphenyl)propyl(diethoxymethyl)phosphinate

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매2회

실험 절차

A solution of 6.5 g of ethyl 2-(4-methylphenyl)-3-nitropropyl(diethoxymethyl)phosphinate in 60 ml of ethanol is added to 52 g of an 8% solution of ammonia in ethanol. To this are added 8 ml of Raney Nickel and the resulting mixture is hydrogenated at 1 bar until the theoretical amount of hydrogen has been taken up. The mixture is then filtered and the filtrate is concentrated under reduced pressure to give ethyl 3-amino-2-(4-methylphenyl)propyl(diethoxymethyl)phosphinate as a viscous oil, 31P=+44.6 ppm (CDCl3).

후처리

  1. filtrationThe mixture is then filtered
  2. concentrationthe filtrate is concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-7c7dcf374f134cf895ad14aa6fc5ddc1
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04656298

반응 노트

불러오는 중…